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| Analytical MethodsUnited States Environmental ProtectionAgencyOffice of Water(4303)Washington, DC 20460EPA-821-F-98-005February 23, 1999Approval of EPA Methods 1664, Revision A, and 9071B for Determination of Oil and Greaseand Non-polar Material in EPA's Wastewater and Hazardous Waste Programs
**Summary**

*EPA announces publication of a final rule approving use of EPA Methods 1664, Revision A, and9071B for determination of oil and grease and non-polar material (NPM) in EPA's wastewaterprogram (40 CFR part 136) and hazardous waste program (40 CFR part 260).  Approval of thesemethods supports EPA's effort to protect Earth's ozone layer by reducing dependency on use ofchlorofluorocarbons (CFCs).  Methods 1664 and 9071B employ n-hexane as the extractionsolvent in place of 1,1,2-trichloro-1,2,2-trifluoroethane (CFC-113), a Class 1 CFC.*

**Background**

The U.S. Environmental Protection Agency (EPA) publishes analytical testing methods thatare used by industrial and municipal facilities to analyze chemical and biological components ofwastewater, drinking water, sediment, and other environmental samples (for the purpose of datagathering and compliance monitoring under the Clean Water Act and the Safe Drinking WaterAct.)

EPA is approving Method 1664, Revision A, for use under the Clean Water Act and as anadditional analytical method for the determination of oil and grease and non-polar material inaqueous matrices in EPA's wastewater and hazardous waste programs. EPA *Method 1664,Revision A: N-Hexane Extractable Material (HEM; Oil and Grease) and Silica Gel Treated N-Hexane Extractable Material (SGT-HEM; Non-polar Material) by Extraction andGravimetry* is being approved as part of EPA's effort to reduce dependency on use ofchlorofluorocarbons (CFCs).  EPA is also approving Method 9071B for use in the hazardouswaste program for solid and semi-solid materials.

**Method 1664, Revision A**

Method 1664, Revision A, is a liquid/liquid extraction (LLE), gravimetric procedure thatemploys normal hexane (*n*-hexane) as the extraction solvent, in place of 1,1,2-trichloro-1,2,2-trifluoroethane (CFC-113; Freon-113), a Class 1 CFC, for determination of theconventional pollutant oil and grease.  Because the nature and amount of material determined isdefined by the solvent and by the details of the method used for extraction, oil and grease andNPM are "method-defined analytes."

Method 1664, Revision A is capable of measuring HEM and NPM in the range of 5 to 1000mg/L, and may be extended to higher levels by analysis of a smaller sample volume collectedseparately.  The method detection limit (MDL) for HEM in Method 1664, Revision A is 1.4mg/L and the minimum level of quantitation (ML) is 5.0 mg/L.

Method 1664, Revision A may be modified to reduce interferences and take advantage ofadvances in technology or to lower the costs of measurements, provided that all methodequivalency and performance criteria are met.  This performance-based approach is consistentwith the Agency's streamlining proposal and the Agency's performance-based measurementsystem policy.

**Improvements and Changes Included in Revision A of Method 1664**

Revision A to Method 1664 is based on comments and analytical data received during bothcomment periods for the proposed rule (61 FR 1730; January 23, 1996 and 61 FR 26149; May24, 1996) and the comment period for the notice of data availability (62 FR 51621; October 2,1997).  The significant improvements include: (1) the term "total petroleum hydrocarbons"(TPH) has been replaced by "non-polar material" (NPM) to avoid confusion with TPHmeasurements by other methods; (2) the requirement for a matrix spike duplicate (MSD) hasbeen changed to a suggestion; (3) the size of an analytical batch has been increased to amaximum of 20 samples per discharge or waste stream; and (4) use of solid-phase extraction(SPE) has been allowed without a demonstration of equivalency, provided that thedischarger/generator assumes the risk associated with any disparity in results from liquid-liquidextraction (LLE).

**Timing of Required Use of Method 1664, Revision A and Phaseout of Use of CFC-113**

EPA proposed to withdraw the currently approved methods six months after publication of thefinal rule in the Federal Register in an effort to provide for use and depletion of existinglaboratory stocks of CFC-113. EPA has decided not to withdraw the CFC-113 based oncommenters' concerns about potentially differing results using the new method that could bring apermittee into noncompliance under certain circumstances.  However, EPA believes that directreplacement of the new method is warranted in most cases.  Therefore, EPA strongly encouragesdischargers/permittees to use Method 1664 rather than the CFC-113 methods for existingpermits.  EPA also recommends the use of the new method for all new permits and reissuedpermits.

**Method 9071B**

EPA is also approving the use of Method 9071B for use in EPA's hazardous waste program. This method is for solid and semi-solid materials.  Method 9071B also uses n-hexane instead ofCFC-113 as the extraction solvent.  This method is not required by any hazardous waste programregulation but it can be included as part of a hazardous waste delisting demonstration.

**Additional Information and Copies**
For more information concerning the final rule approving use of Method 1664, Revision A ,please contact Dr. Maria Gomez-Taylor, in EPA's Office of Water (4303), USEPA Office ofScience and Technology, 401 M Street, SW, Washington, DC 20460, (Phone:  202-260-1639);E-mail: [email protected]).  Forinformation regarding the use of Method 1664, Revision A in the Office of Solid Waste, contactGail Hansen, in EPA's Office of Solid Waste (5307W), USEPA, 401 M Street, SW, Washington,DC 20460, (703-308-8855; E-mail: [email protected]).  The final rule published in the *Federal Register*contains instructions on how to obtain additional information and how to review the publicrecord for this rulemaking.

The complete text of the *FederalRegister* notice containing this final rule may beaccessed through the Internet and the Superintendent of Documents homepage at http://www.access.gpo.gov/su_docs/.  The fulltext of EPA Method 1664, Revision A may be viewed or downloaded from the Internet at http://www.epa.gov/waterscience/guide.
You may also obtain copies of Method 1664, Revision A through the U.S. EPA National ServiceCenter for Environmental Publications (NSCEP), 11029 Kenwood Road, Cincinnati, OH 45242. Method 1664, Revision A will also be made available at the National Technical InformationService (NTIS), 5285 Port Royal Road, Springfield, VA 22161, (703)605-6000 or (800)553-6847. The NTIS number is PB99-121949.

 

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